CN104874813A - Preparation method of ultrathin super-long silver nanowire - Google Patents
Preparation method of ultrathin super-long silver nanowire Download PDFInfo
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- CN104874813A CN104874813A CN201510282193.9A CN201510282193A CN104874813A CN 104874813 A CN104874813 A CN 104874813A CN 201510282193 A CN201510282193 A CN 201510282193A CN 104874813 A CN104874813 A CN 104874813A
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Abstract
The invention relates to a preparation method of an ultrathin super-long silver nanowire, which comprises the steps: sequentially placing polyvinylpyrrolidone PVP and silver nitrate into a reaction container; adding a solvent; carrying out stirring until the PVP and the silver nitrate are completely dissolved; then adding ascorbic acid; performing the reaction for 1 to 24 hours at a temperature of 50 to 100 DEG C to obtain the ultrathin super-long silver nanowire. The method disclosed by the invention is simple and convenient to operate; experimental facilities are simple; raw materials are easy to obtain; the reaction temperature is low; cost is low. The silver nanowire prepared by the method has very wide prospect in the field of a transparent conductor and application.
Description
Technical field
The invention belongs to the preparation field of nano silver wire, particularly a kind of preparation method of ultra-fine ultra-long silver nanowire.
Background technology
Nano silver wire, except having the excellent electric conductivity of silver, due to the dimensional effect of Nano grade, also has excellent light transmission, flexible resistance.Therefore being considered to be the most possible material substituting conventional I TO transparent conductor, providing possibility for realizing flexibility, bent LED display, touch-screen etc., and existing large quantifier elimination is applied to thin-film solar cells.
Nano silver wire is as the performance of transparent conductor by the impact of diameter and draw ratio, and diameter is less, and draw ratio is larger, its performance better (ACS Nano 2013,7, (9), 7654-63; Nanoscale 2012,4,1996.).In the preparation method of nano silver wire, research method the most thorough is reduction of ethylene glycol method.The nano silver wire diameter that this method obtains is substantially all at more than 30nm, and draw ratio is below 1500.Its needs the reproducibility ensureing ethylene glycol under higher than 100 DEG C of conditions, even if also can not get nano silver wire (Chem.Mater.2002,14,4736) at 100 DEG C of reaction 20h.Therefore, the new preparation method of research and development is needed to obtain ultra-fine ultra-long silver nanowire.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of ultra-fine ultra-long silver nanowire, the method raw material is easy to get, simple to operate, the nano silver wire prepared its to be used as transparency electrode be the excellent performance of performance: at transmitance T550=98.7% place, face hinders and is low to moderate 90 ohm.
The preparation method of a kind of ultra-fine ultra-long silver nanowire of the present invention, comprising:
Polyvinylpyrrolidone PVP and silver nitrate are put into reaction vessel successively, adds solvent, be stirred to and dissolve completely, then add ascorbic acid, at 50-100 DEG C, react 1-24h; Wherein, the mol ratio of polyvinylpyrrolidone PVP, silver nitrate and ascorbic acid is 2-6:1:0.02-0.1.
The molecular weight >55K of described PVP.
Described ascorbic acid is reducing agent.
In described preparation method, before adding solvent, micro ion can be added in reaction vessel, the amount≤0.66mol added of micro ion.
Described micro ion is chlorion, bromide ion, iodide ion or iron ion.
Described solvent is water or ethylene glycol.
The present invention utilizes ascorbic acid as reducing agent, and having obtained average diameter is 20nm, draw ratio up to 2000 nano silver wire.Meanwhile, it is used as transparency electrode, at transmitance T550=98.7% place, face resistance is low to moderate 90 ohm.
The present invention for raw material, can prepare ultra-fine ultra-long silver nanowire with simple experimental provision with common predecessor, can be used as excellent transparency electrode.The advantages such as this reaction has environmental friendliness, required raw material are easy to get, cheap, operating process is easy.
beneficial effect
(1) method raw material of the present invention is easy to get, cheap, and experimental provision is simple, and reaction temperature is low, easy and simple to handle;
(2) the ultra-fine ultra-long silver nanowire for preparing of the present invention, average diameter is 20nm, and draw ratio is up to 2000;
(3) the ultra-fine ultra-long silver nanowire that the present invention prepares is used as excellent transparency electrode, at transmitance T
550=98.7% place, face resistance is low to moderate 90 ohm.
Accompanying drawing explanation
Fig. 1 is the high power scanning electron microscope (SEM) photograph of the nano silver wire of preparation in embodiment 3;
Fig. 2 is the light microscope figure of the nano silver wire of preparation in embodiment 3;
Fig. 3 is the low power scanning electron microscope (SEM) photograph of the nano silver wire of preparation in embodiment 3;
Fig. 4 is the transmitance of nano silver wire as the transparency electrode-face resistance curve of preparation in embodiment 3.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Preparation following solutions: NaCl is the aqueous solution or the ethylene glycol solution of 0.2M, and ascorbic acid is the aqueous solution or the ethylene glycol solution of 0.1M.
Embodiment 2
In flask, add 0.3g PVP, 0.21g silver nitrate successively, add 10mL deionized water, after fully stirring, add the 0.2mL aqueous ascorbic acid of preparation in embodiment 1 wherein, at 100 DEG C, react 14h.
Embodiment 3
In flask, add 0.3g PVP, 0.21g silver nitrate successively, add 10mL deionized water, after fully stirring, add the aqueous solution of 10 μ LNaCl of preparation in embodiment 1 wherein, 0.2mL aqueous ascorbic acid, reacts 24h at 100 DEG C.Fig. 1-4 is the data obtained under this condition.As can be seen from the figure nanowire diameter is 20nm (Fig. 1), and length reaches 50 μm (Fig. 2,3); This nanowire dispersion is layered at the bottom of glass substrate by Meyer rod mode and obtains transparency electrode, its performance again 98.7% transmitance below resistance be low to moderate 90 ohm.
Embodiment 4
In flask, add 0.3g PVP, 0.21g silver nitrate successively, add 10mL ethylene glycol, after fully stirring, add 0.2mL ascorbic acid ethylene glycol solution wherein, at 80 DEG C, react 10h.
Claims (3)
1. a preparation method for ultra-fine ultra-long silver nanowire, comprising:
Polyvinylpyrrolidone PVP and silver nitrate are put into reaction vessel successively, adds solvent, be stirred to and dissolve completely, then add ascorbic acid, at 50-100 DEG C, react 1-24h; Wherein, the mol ratio of polyvinylpyrrolidone PVP, silver nitrate and ascorbic acid is 2-6:1:0.02-0.1.
2. the preparation method of a kind of ultra-fine ultra-long silver nanowire according to claim 1, is characterized in that, before adding solvent, in reaction vessel, adds micro ion, the amount≤0.66mol added of micro ion.
3. the preparation method of a kind of ultra-fine ultra-long silver nanowire according to claim 2, is characterized in that, described micro ion is chlorion, bromide ion, iodide ion or iron ion.
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Cited By (5)
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CN105537613A (en) * | 2015-12-25 | 2016-05-04 | 蚌埠玻璃工业设计研究院 | Microwave-assisted hydrothermal method for preparing long silver nanowires |
CN106601914A (en) * | 2016-12-22 | 2017-04-26 | 东南大学 | Method for preparing polycrystalline ultra-thin metal film and two-dimensional nano pattern |
CN110586931A (en) * | 2019-10-30 | 2019-12-20 | 哈尔滨工业大学 | Ultra-long silver nanowire and preparation method thereof |
CN110640163A (en) * | 2019-10-18 | 2020-01-03 | 上海交通大学 | Method for preparing superfine silver nanowires with ultrahigh length-diameter ratio |
CN111032257A (en) * | 2017-08-09 | 2020-04-17 | 同和电子科技有限公司 | Method for manufacturing silver nanowire, silver nanowire ink, and transparent conductive film |
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CN103752850A (en) * | 2014-02-18 | 2014-04-30 | 南京瑞盈环保科技有限公司 | Method for utilizing alumina template to manufacture silver nanowires |
CN104313687A (en) * | 2014-07-16 | 2015-01-28 | 浙江坦福纳米科技有限公司 | Preparation technology of silver nanowires with small diameter and high length-diameter ratio |
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KR101337412B1 (en) * | 2011-10-26 | 2013-12-06 | 고려대학교 산학협력단 | Manufacturing method for metal nanowire in room temperature and aqueous media |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105537613A (en) * | 2015-12-25 | 2016-05-04 | 蚌埠玻璃工业设计研究院 | Microwave-assisted hydrothermal method for preparing long silver nanowires |
CN106601914A (en) * | 2016-12-22 | 2017-04-26 | 东南大学 | Method for preparing polycrystalline ultra-thin metal film and two-dimensional nano pattern |
CN111032257A (en) * | 2017-08-09 | 2020-04-17 | 同和电子科技有限公司 | Method for manufacturing silver nanowire, silver nanowire ink, and transparent conductive film |
CN110640163A (en) * | 2019-10-18 | 2020-01-03 | 上海交通大学 | Method for preparing superfine silver nanowires with ultrahigh length-diameter ratio |
CN110640163B (en) * | 2019-10-18 | 2021-11-30 | 上海交通大学 | Method for preparing superfine silver nanowires with ultrahigh length-diameter ratio |
CN110586931A (en) * | 2019-10-30 | 2019-12-20 | 哈尔滨工业大学 | Ultra-long silver nanowire and preparation method thereof |
CN110586931B (en) * | 2019-10-30 | 2022-03-08 | 哈尔滨工业大学 | Ultra-long silver nanowire and preparation method thereof |
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Application publication date: 20150902 |